Classifications

• • G—PHYSICS
  • G01—MEASURING; TESTING
  • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
  • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
  • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
  • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
  • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
  • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
  • G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor

Definitions

• the present invention relates to an apparatus and a process for measuring bulk material properties flowing in a pipe by light reflection and to the use of this apparatus.
• a pipe When a pipe is provided with a light transmissible window it is possible to perform measurements of the bulk material flowing in the pipe, such as powder size, colours, chemical compositions, chemical and physical properties etc. by using light, such as UN, visible or IR-light.
• light such as UN, visible or IR-light.
• ⁇ IR is a subregion of IR light and to measure the near infrared ( ⁇ IR) spectrum of a polyolefin powder in a pneumatic or gravity transport pipe a sapphire window was inserted in the pipe wall and an analyser was provided outside the window which emits and measures the IR- radiation reflected by the bulk material inside the pipe.
• ⁇ IR near infrared
• DE4014739C2 discloses an apparatus for measuring the light absorption of solid particles in a liquid flowing in a pipe by light transmission.
• the apparatus has a curved pipe section.
• the measurement element is mounted in a region of the curved section in which higher flow speeds occur than in other regions to prevent solid deposits between the emitter which transmits the light through the liquid to the opposite detector of the measurement element.
• This object is attained by using a pipe with an elbow, at least one window in a plate or a flat surface at the outside of the elbow and a light reflection analyser outside the window, so that light sent through the window is reflected by the bulk material and measured by the analyser detector, the plate being arranged in such a way between the entrance side and the exit side of the elbow that the bulk material incoming from the entrance side is deflected by the plate to the exit side of the elbow.
• the elbow is preferably an elbow for connecting two pipes at an angle of 90°, particularly an elbow according to US-A-5288111, that is a 90° elbow adapted for use in a transport pipe and defining an inner elbow side and an outer elbow side, comprising: a first pipe section or socket for attachment of a pipe; a first pipe portion defining an axis and being connected to said pipe section, said first pipe section including a flared pipe shell extending at the inner elbow side to provide said first pipe section with a cross- sectional expansion expanding in a direction away from said first pipe section; a pipe bend including a quadrantal pipe shell connected to said flared pipe shell at the inner elbow side; a second pipe section including a cylindrical shell which is connected to said quadrantal pipe shell at said inner elbow side, and a tapered pipe shell connected to said cylindrical shell at the outer elbow side to provide said second pipe section with a cross- sectional contraction contracting in a direction away from said quadrantal pipe shell; said pipe bend further including a baffle plate arranged between said first pipe section
• elbows are possible.
• the elbow according to US-A-5288111 is particularly preferred, because the light transmissible window can easily be inserted in the baffle plate to form a window for light reflection measurement, and because the impact of the product on the baffle plate guarantees firstly a measurement made on full representative product sample as a moving product layer is built up which is presented for light reflection and secondly a self cleaning effect of the window.
• the elbow may have another angle.
• the light-transmissible window at the outside of the elbow at which the reflection analyser is mounted is arranged at an angle between more than 30° and less than 80° to the axis of the first pipe section.
• the plate has to be inclined to the axis of the pipe section at the entrance side, preferably at an angle of at least 20° smaller than the angle between the axes of the first and the second pipe sections.
• the window plate is preferably arranged at an angle between 55° and 65° to the axis of the first pipe section.
• the cross-section of the elbow increases from the first pipe section to the plate in the 90° elbow.
• the first pipe portion between the first pipe section and the window plate includes a flared pipe shell extending at the inner elbow side expanding in a directional way from the first pipe section.
• the first and the second pipe section of the elbow may be arranged at the same height or at a different height.
• the pipe axis of the first section at the entrance side of the elbow as well as the pipe axis of the second section and the axis side may lie in the same horizontal plane or in case of a 90° elbow the axis of the first pipe section may be arranged horizontally and the pipe axis of the second section vertically.
• the bulk material incoming from the entrance side of the elbow is deflected by the window plate to the exit side of the elbow to build a continuous moving layer in front of the window, so flat that an effective reflective light-spectrum can be obtained.
• the impact of the bulk material on the window plate has a self-cleaning effect.
• the light used for measurement according to the invention can be any light or radiation reflected by the bulk material which passes the window. That is UV, visible light, or IR-light can be used to perform all kinds of measurements which are possible through a window in the baffle plate of the elbow, such as particle size, colours, chemical compositions, chemical and physical properties etc.
• the invention is particularly suitable for measuring bulk material flowing in a pipe by IR-spectroscopy that is, in particular, for granulate, powder or pellet material.
• the at least one window consists of IR- transmissible material and the analyser emits IR-radiation and measures the IR-radiation reflected by the bulk material in the pipe.
• the IR-analyser arranged outside the window or baffle plate can be any analyser used for reflection IR-spectroscopy of solids, in particular a commercial NIR reflection IR-analyser.
• a reflection IR-analyser one can use an AOTF (acousto-optical tunable filter) spectrometer for instance.
• the bulk material to be measured with the apparatus according to the present invention can be any bulk material, in particular bulk material in form of powder, granules, or pellets.
• the bulk material may have any particle size being used in pneumatic transport systems.
• As conveying gas for the pneumatic transport system for instance air, nitrogen, oxygen, propane, propylene and mixtures of these gases can be used.
• the volume ratio of the solids of the bulk material to the gas in the pipe is preferably 1 : 10 to 50:1, in particular 1 : 1 to 8: 1.
• the apparatus of the present invention can be used to measure physical or chemical properties of inorganic or organic bulk materials flowing in a pipe by light reflection using UN, visible or IR light, that is in particular from 10 "8 to 10 "1 cm, preferably from 10 "5 to 10 "2 cm. All kinds of light reflection can be used, including fluorescence and Raman spectroscopy. It is particularly usable for IR-analysis, in particular ⁇ IR subregion of the IR region. For instance, the quality of bulk material may be controlled. In particular in a process in which bulk material is produced the bulk material may be analyzed in accordance with the present invention. Such a process is, for instance, a polymerization process in which the polymer is obtained in form of bulk material. A particularly preferred use of the present invention is the analysis of polyolefins, such as polymers or copolymers of ethylene or propylene.
• the pipe in which the elbow is inserted may have any inner diameter suitable for pneumatic transport application.
• flushing can be omitted when the inner diameter of the first section at the inlet of the elbow is restricted by a conical reducing baffle which speeds up the stream of bulk material so that the material is brought in motion in front of the windows. That means, by reducing the inner diameter of at least the first pipe section the problem of blocking the window at the start can be overcome.
• the flow of materials depends on the right flow pattern, mass flow and speeds.
• proper flowing and formation of the moving product layer in front of the window can be modified by changing the diameter of the entrance pipe to the gamma bend and/or by flushing the gamma bend by transport gas.
• Figure 1 is a perspective illustration of an apparatus according to the present invention
• Figure 2 is a schematic longitudinal section of the apparatus of figure 1 ;
• Figure 3 is a plan view of the window
• Figure 4 are NIR-spectra.
• an elbow for connecting pipes (not shown) at an angle of 90° includes a cylindrical pipe socket or section 1 which is pro- vided with a flange 2 for attachment to one pipe.
• pipe section 1 is connected to a first pipe portion 3.
• the first pipe portion 3 has a cylindrical shell 4 extending at the outer elbow side and connected to a flared upper shell 5 at the inner elbow side.
• the first pipe portion 3 has a continuously expanding cross- sectional area in flow direction indicated by arrow 6.
• a pipe bend 7 including a quadrantal pipe shell 8 at the inner elbow arch and a baffle plate 9 at the outer elbow arch in opposition to pipe shell 8.
• Baffle plate 9 is connected with a number of suitable segments to quadrantal pipe shell 8 to form a closed cross-sectional area.
• the pipe bend 7 is followed by a second pipe portion 11 which includes a cylindrical shell
• Pipe portion 11 ends in a diameter corresponding to the nominal diameter of a following pipe socket or section
• the cone angle of the conical shell 5 and/or the length of the first pipe portion 3 are selected in such a manner that the bulk material particles 17 transported along arrows 6 always detach from the wall surface in the area of the first pipe portion 3. Moreover, the conveying speed is diminished by means of this cross-sectional extension.
• a disc 18 Tightly fixed in a cut-out of plate 9 is a disc 18 provided with tightly fixed discs or plates 24a, 24b, and 24c of NIR-transmissible material (figure 3) which serve as windows for reflection IR-spectroscopy with an NIR- spectrometer or analyser 19 (from which a part is broken away in figure 1).
• Plate 9 is arranged at an angle ⁇ between 55° and 65° relative to the axis 21 of the first pipe section 1 at the entrance side of the elbow. Because the angle between the axis 21 of the first pipe section and the axis 22 of the second pipe section 14 is 90°, angle ⁇ is about 25 to 35 degrees smaller.
• disc 18 is tightly fixed with bolts 23 to plate 9.
• window 24a is arranged in the center of disc 18, whereas the other discs 24b and 24c are radially offset in a different direction and at a different distance from the center.
• One or more discs 24a, 24b, and 24c are provided because the optimum particle flow is unpredictable. However, it is also possible to provide windows which reach nearly the entire area of the disk or cover 18. A very fair and dense flow of a bulk material is attained with window 24a at a 12 o'clock location.
• the diameter D at the outlet side of the first pipe portion 3 is about 1.2 to 1.5 times the diameter d at the entrance side of the first pipe portion 3.
• the distance a between the leading edge of the entrance side of plate 9 and the exit side of the first pipe portion 3 corresponds at least to diameter D.
• the plate 9 is spaced from the quadrantal pipe shell by a minimum distance a which does not significantly exceed diameter D.
• Plate 9 has a length 1 which corresponds to about 1.5 times to 2 times diameter d.
• the second pipe portion 1 1 is designed in the same manner as the first pipe portion 3, i.e. with the same configuration and same dimensions.
• a diameter reducing funnel 25 can be inserted in the first pipe portion 3 for accelerating the flow speed.
• a gas inlet pipe 26 can be provided in the first pipe portion 3 directed to baffle plate 9 to enable long or short term changes of the flow pattern.
• typical operation conditions are for example as follows: Pick-up conditions: about 50 to about 90°C against about 0,2 to about 1 barg, in particular about 70°C against about 0,45barg.
• Product throughput about 5 to 80 t/h, in particular about 25,5 t/h
• Solids to air ratio about 1.0 to 3.0, in particular about 1.6
• Product speed at the elbow inlet 10 to about 60m/sec, in particular about 30m/sec.
• Product speed at the reducing baffle outlet 20 to 60 m/sec, in particular about 40m/sec.
• an NIR-spectrum is collected.
• windows 24a, 24b, 24c one uses sapphire windows.
• the inner diameter of the first and second pipe sections 1 and 14 are 356 mm (12 inches), respectively.
• spectrum A shows a significant improvement of the signal to noise ratio compared with spectrum B.

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• Physics & Mathematics (AREA)
• Spectroscopy & Molecular Physics (AREA)
• Biochemistry (AREA)
• Life Sciences & Earth Sciences (AREA)
• Chemical & Material Sciences (AREA)
• Analytical Chemistry (AREA)
• Health & Medical Sciences (AREA)
• General Health & Medical Sciences (AREA)
• General Physics & Mathematics (AREA)
• Immunology (AREA)
• Pathology (AREA)
• Investigating Or Analysing Materials By Optical Means (AREA)
• Measuring Volume Flow (AREA)
• Optical Measuring Cells (AREA)

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• 2000
  • 2000-12-28 US US10/250,450 patent/US20040065830A1/en not_active Abandoned
  • 2000-12-28 JP JP2002554700A patent/JP2004517317A/ja active Pending
  • 2000-12-28 WO PCT/EP2000/013312 patent/WO2002054048A1/en not_active Application Discontinuation
  • 2000-12-28 CN CNA008201072A patent/CN1479865A/zh active Pending
  • 2000-12-28 CA CA002432182A patent/CA2432182A1/en not_active Abandoned
  • 2000-12-28 BR BR0017397-5A patent/BR0017397A/pt not_active IP Right Cessation
  • 2000-12-28 EP EP00988808A patent/EP1346202A1/en not_active Withdrawn

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